色谱

色谱 ›› 2015, Vol. 33 ›› Issue (9): 943-945.DOI: 10.3724/SP.J.1123.2015.04003

• 亲水作用色谱专栏 • 上一篇    下一篇

亲水作用色谱-串联质谱法测定乳及乳制品中左旋肉碱

刘艳明1, 薛霞1, 刘国强2, 任雪梅1, 胡梅1, 祝建华1   

  1. 1. 山东省食品药品检验研究院, 山东 济南 250101;
    2. 国家电网公司山东省电力公司电力科学研究院, 山东 济南 250002
  • 收稿日期:2015-04-02 出版日期:2015-09-08 发布日期:2015-09-09
  • 通讯作者: 刘艳明

Determination of L-carnitine in milk and dairy products by hydrophilic liquid chromatography-tandem mass spectrometry

LIU Yanming1, XUE Xia1, LIU Guoqiang2, REN Xuemei1, HU Mei1, ZHU Jianhua1   

  1. 1. Shandong Institute for Food and Drug Control, Ji'nan 250101, China;
    2. Shandong Electric Power Research Institute of Shandong Electric Power Company, State Grid Corporation of China, Ji'nan 250002, China
  • Received:2015-04-02 Online:2015-09-08 Published:2015-09-09

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127

被引次数

2

摘要：

建立了亲水作用色谱-串联四极杆质谱测定乳及乳制品中左旋肉碱的分析方法。样品经2%(v/v)乙酸水溶液提取、乙腈沉淀蛋白质净化,以乙酸铵和乙腈为流动相,经Acquity UPLC BEH HILIC色谱柱分离后采用电喷雾质谱多反应监测(MRM)方式扫描,外标法定量。结果表明,左旋肉碱的质量浓度在1~100 μg/L范围内线性关系良好(r2> 0.99),定量限为0.01 mg/kg。标准加入法测定左旋肉碱在高、中、低3个加标水平的回收率为96.0%~103.4%,相对标准偏差(RSD)为1.2%~4.3%。该方法前处理简单、快速,检测结果准确、灵敏,可为各类乳及乳制品中左旋肉碱的含量水平测定、研究和控制提供技术支持。

关键词: 亲水作用色谱-串联质谱, 乳, 乳制品, 左旋肉碱

Abstract:

An analytical method was developed for the determination of L-carnitine in milk and dairy products using hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/MS). The samples were extracted with 2%(v/v) acetic acid solution, and the protein was precipitated with acetonitrile subsequently. The separation of L-carnitine was carried out on an Acquity UPLC BEH HILIC column using ammonium acetate and acetonitrile as mobile phases. The quantification analysis of the target compound was performed under multiple reaction monitoring (MRM) mode by external standard method. A good linear relationship was obtained between the peak area and concentration of L-carnitine in the range of 1-100 μg/L with the correlation coefficient more than 0.99. The limit of quantification (LOQ) of L-carnitine was 0.01 mg/kg. The spiked recoveries were 96.0%-103.4%. The precisions (RSDs) were 1.2%~4.3%. The sample preparation was simple and rapid, and the results were precise and sensitive. The developed method is suitable for the study of concentration of L-carnitine in milk and dairy products, and the technical support for the infant formula is provided.

Key words: dairy products, hydrophilic liquid chromatography-tandem mass spectrometry (HILIC-MS/MS), L-carnitine, milk

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